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One-step preparation method for high nitrogen doped graphene

A graphene and high nitrogen technology, which is applied in the field of one-step preparation of high nitrogen doped graphene, can solve the problems of difficulty in realizing industrial mass production, complicated preparation process, low nitrogen doping amount, etc., and achieves low price and low preparation technology. Simple, low production cost effect

Inactive Publication Date: 2016-03-23
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the common synthesis method of nitrogen-doped graphene is roughly to use the graphite layer for physical or chemical treatment to obtain a separated layered structure, and at the same time add a suitable nitrogen source to realize the nitrogen doping of graphene during the synthesis process, specifically including graphite oxide Chemical reduction method, chemical vapor deposition method and solvothermal method, etc. However, most of these methods have defects such as complex preparation process, low yield and high cost, it is difficult to achieve industrial mass production, and there is also the problem of low nitrogen doping amount

Method used

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  • One-step preparation method for high nitrogen doped graphene
  • One-step preparation method for high nitrogen doped graphene
  • One-step preparation method for high nitrogen doped graphene

Examples

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Effect test

Embodiment 1

[0028] (1) Dissolve 6 g of urea and 0.3 g of sucrose in 20 mL of deionized water, stir to obtain an aqueous solution, and dry the above solution to obtain a white powder;

[0029] (2) The white powder is placed in a tube furnace, heated to 300° C. in a nitrogen atmosphere at a heating rate of 4° C. / min, kept for 1 hour, and the gas flow rate is 40 sccm;

[0030] (3) Continue to increase the calcination temperature to 900° C. at a heating rate of 8° C. / min and keep it warm for 2 hours, and keep the nitrogen flow rate at 40 sccm;

[0031] (4) After calcination, the black product was cooled to room temperature under the protection of nitrogen, and high nitrogen-doped graphene was obtained after grinding. figure 1 The scanning electron microscope image of high nitrogen-doped graphene prepared for this example shows an obvious curly layered structure accompanied by a large number of undulating wrinkles. figure 2 The transmission electron microscope image of high nitrogen-doped gr...

Embodiment 2

[0038] (1) Dissolve 6g of dicyandiamide and 0.3g of fructose in 20mL of deionized water, stir to obtain an aqueous solution, and dry the above solution to obtain a white powder;

[0039] (2) The white powder is placed in a tube furnace, heated to 300° C. in a nitrogen atmosphere at a heating rate of 4° C. / min, kept for 1 hour, and the gas flow rate is 40 sccm;

[0040] (3) Continue to increase the calcination temperature to 900° C. at a heating rate of 8° C. / min and keep it warm for 2 hours, and keep the nitrogen flow rate at 40 sccm;

[0041] (4) After calcination, the black product was cooled to room temperature under the protection of nitrogen, and high nitrogen-doped graphene was obtained after grinding. In the scanning electron microscope image of the high nitrogen-doped graphene prepared in this example, an obvious curly layered structure can be observed, accompanied by a large number of undulating wrinkles. The high-nitrogen-doped graphene prepared in this example show...

Embodiment 3

[0048] 1) Dissolve 6g of dicyandiamide and 0.3g of fructose in 20mL of deionized water, stir evenly to obtain an aqueous solution, and dry the above solution to obtain a white powder;

[0049] (2) The white powder is placed in a tube furnace, heated to 300° C. in a nitrogen atmosphere at a heating rate of 4° C. / min, kept for 1 hour, and the gas flow rate is 40 sccm;

[0050] (3) Continue to increase the calcination temperature to 1000° C. at a heating rate of 8° C. / min and keep it warm for 2 hours, and the nitrogen flow rate remains at 40 sccm;

[0051] (4) After calcination, the black product was cooled to room temperature under the protection of nitrogen, and high nitrogen-doped graphene was obtained after grinding. In the scanning electron microscope image of the high nitrogen-doped graphene prepared in this example, an obvious curly layered structure can be observed, accompanied by a large number of undulating wrinkles. The high-nitrogen-doped graphene prepared in this ex...

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Abstract

The invention discloses a preparation method of high nitrogen doped graphene. The method comprises the following steps of: using a nitrogen source and a carbon source as raw materials, and carrying out effective mixing and drying to obtain a mixture; putting the mixture in an inert atmosphere, warming and heating the mixture to 300-600 DEG C, and carrying out heat preservation for a period of time; then continuously heating the mixture to 700-1200 DEG C, and carrying out heat preservation for a period of time to finally generate a black solid, namely the high nitrogen doped graphene. The preparation method disclosed by the invention is simple in process; the high-quality nitrogen doped graphene is obtained through a solid-phase reaction one-step method; and the nitrogen doped graphene is easy for industrial mass production. Moreover, the material has many nitrogen doped active sites, and has good electro-catalysis oxygen reduction activity as a non-noble metal catalyst.

Description

technical field [0001] The invention relates to the one-step preparation of high nitrogen-doped graphene. Background technique [0002] High-nitrogen-doped graphene has excellent electrical, optical, thermal and mechanical properties, and has gradually become a research hotspot in the field of science. It has broad applications in the fields of nano-microelectronics, gas sensors, catalyst carriers, photoelectric conversion and energy storage materials. prospect. For example, nitrogen atoms are doped in the graphene lattice and at the edge, and a large number of holes can be formed after calcination in an inert atmosphere, and the surface is rich in pyridine-type and pyrrole-type nitrogen doping atoms. Theoretical simulation calculations show that this high nitrogen-doped graphene has additional lithium storage properties (Nat. Commun. 2014, 5, 5261). Compared with pure graphene, high nitrogen-doped graphene, as a non-noble metal catalyst for electrocatalytic oxygen reducti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 曹敏花秦锦雯王曙光
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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